UPLC波长切换法同时测定心通颗粒中7个成分的含量  

Simultaneous determination of seven components in Xintong granules by UPLC wavelength switching method

作　　者：庄会芳 袁晓梅 庄建林 赵森森 范建伟 张贵民 ZHUANG Hui-fang;YUAN Xiao-mei;ZHUANG Jian-lin;ZHAO Sen-sen;FAN Jian-wei;ZHANG Gui-min(Lunan Pharmaceutical Group Co.,Ltd.,State Key Laboratory of Generic Manufacture Technology of Chinese Traditional Medicine,Linyi 276006,China;Lunan Hope Pharmaceutical Co.,Ltd.,Linyi 276006,China)

机构地区：[1]鲁南制药集团股份有限公司,中药制药共性技术国家重点实验室,临沂276006 [2]鲁南厚普制药有限公司,临沂276006

出　　处：《药物分析杂志》2023年第8期1284-1290,共7页Chinese Journal of Pharmaceutical Analysis

基　　金：山东省重点研发计划(重大科技创新工程)项目(2020CXGC010505,2021CXGC010508);山东省新旧动能转换重大产业攻关项目(鲁动能办[2021]23号)。

摘　　要：目的:建立同时测定心通颗粒中葛根素、大豆苷、2,3,5,4’-四羟基二苯乙烯-2-O-β-D-葡萄糖苷、柚皮苷、丹酚酸B、淫羊藿苷和丹参酮ⅡA 7个成分含量的方法。方法:采用UPLC波长切换法,色谱柱为Waters CORTECSⓇC_(18)柱(50 mm×4.6 mm,2.7μm),流动相为乙腈(A)-0.1%磷酸水溶液(B),梯度洗脱,流速0.3~0.5 mL·min^(-1),柱温35℃,检测波长250 nm(0~15 min时,检测葛根素和大豆苷)、320 nm(15~23 min时,检测2,3,5,4’-四羟基二苯乙烯-2-O-β-D-葡萄糖苷)、283 nm(23~36 min时,检测柚皮苷和丹酚酸B)、270 nm(36~56 min时,检测淫羊藿苷和丹参酮ⅡA)。结果:葛根素、大豆苷、2,3,5,4’-四羟基二苯乙烯-2-O-β-D-葡萄糖苷、柚皮苷、丹酚酸B、淫羊藿苷和丹参酮ⅡA质量浓度分别在34.43~344.32μg·mL^(-1)(r=0.9999)、8.33~83.28μg·mL^(-1)(r=0.9999)、1.48~14.76μg·mL^(-1)(r=0.9999)、2.37~23.68μg·mL^(-1)(r=0.9998)、14.58~145.76μg·mL^(-1)(r=0.9999)、1.86~18.56μg·mL^(-1)(r=0.9999)、0.62~6.24μg·mL^(-1)(r=0.9999)与峰面积的线性关系良好;平均加样回收率(n=6)分别为98.9%,98.3%,98.1%,98.2%,98.6%,99.1%和98.2%,RSD均小于1.5%。24批心通颗粒供试样品中,上述葛根素等7个成分的含量测定结果(n=6)依次为7.813~8.338、1.834~2.119、0.336~0.405、0.611~0.764、3.018~3.753、0.445~0.554和0.139~0.174 mg·g^(-1)。结论:建立的UPLC波长切换法快速、简便而准确,可用于心通颗粒的质量控制。Objective:To establish a quantitative method for simultaneous determination of puerarin,daidzin,2,3,5,4’-tetrahydroxystilbene-2-O-β-D-glucoside,naringin,salvianolic acid B,icariin and tanshinoneⅡA in Xintong granules.Methods:UPLC wavelength switching method was adopted in the assay.The chromatographic analysis was performed on a Waters CORTECSⓇC_(18)column(50 mm×4.6 mm,2.7μm),and the mobile phase was acetonitrile(A)-0.1%phosphoric acid solution(B)with gradient elution.The flow rate was 0.3-0.5 mL·min^(-1),and the column temperature was 35℃.The detection wavelength was chosen at 250 nm for puerarin and daidzin during 0-15 min,320 nm for 2,3,5,4’-tetrahydroxystilbene-2-O-β-D-gluco⁃side during 15-23 min,283 nm for naringin and salvianolic acid B during 23-36 min,and 270 nm for icariin and tanshinoneⅡA during 36-56 min.Resluts:Satisfactory linearities of puerarin,daidzin,2,3,5,4’-tetrahydrox⁃ystilbene-2-O-β-D-glucoside,naringin,salvianolic acid B,icariin and tanshinoneⅡA were in the ranges of 34.43-344.32μg·mL^(-1)(r=0.9999),8.33-83.28μg·mL^(-1)(r=0.9999),1.48-14.76μg·mL^(-1)(r=0.9999),2.37-23.68μg·mL^(-1)(r=0.9998),14.58-145.76μg·mL^(-1)(r=0.9999),1.86-18.56μg·mL^(-1)(r=0.9999)and 0.62-6.24μg·mL^(-1)(r=0.9999),respectively.The average recoveries(n=6)were 98.9%,98.3%,98.1%,98.2%,98.6%,99.1%and 98.2%,respectively,with RSDs less than 1.5%.The contents ranges of puerarin and other 6 components in 24 batches of Xintong granules samples were 7.813-8.338 mg·g^(-1),1.834-2.119 mg·g^(-1),0.336-0.405 mg·g^(-1),0.611-0.764 mg·g^(-1),3.018-3.753 mg·g^(-1),0.445-0.554 and 0.139-0.174 mg·g^(-1),respectively.Conclusion:The UPLC wavelength switching method established is rapid,simple and accurate,which can be used for the quality control of Xintong granules.

关 键 词：心通颗粒 葛根素 大豆苷 2 3 5 4’-四羟基二苯乙烯-2-O-β-D-葡萄糖苷 柚皮苷 丹酚酸B 淫羊藿苷 丹参酮ⅡA 超高效液相色谱 

分 类 号：R917[医药卫生—药物分析学]